CN108172842B - Preparation method of three-element double-layer PdNi @ Pt nanowire - Google Patents

Preparation method of three-element double-layer PdNi @ Pt nanowire Download PDF

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CN108172842B
CN108172842B CN201711420474.1A CN201711420474A CN108172842B CN 108172842 B CN108172842 B CN 108172842B CN 201711420474 A CN201711420474 A CN 201711420474A CN 108172842 B CN108172842 B CN 108172842B
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高发明
于丹
陶璐
杨云霞
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Yanshan University
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Abstract

A three-element bimetallic core-shell structure nanowire is a one-dimensional core-shell structure nanowire which is formed by wrapping a layer of Pt on a PdNi alloy nanowire with the diameter of 4.8 nm. The preparation method of the three-element bimetallic core-shell structure nanowire mainly comprises the steps of preparing the PdNi alloy nanowire with the diameter of 4.8nm by a hydrothermal solvent method, mixing a PdNi alloy nanowire solution with an ethylene glycol solvent, stirring by magnetic force, and then dropwise adding H by using a liquid-transferring gun2PtCl6And stirring for 8-12 h at 50-80 ℃, finally centrifugally cleaning for 2-3 times by using ethanol at 8000-9500 r/min, and drying in a 70 ℃ blast drying oven to obtain the ternary double-layer PdNi @ Pt nanowire. The method is simple, the cost of the catalyst is reduced, and the activity of the catalyst is greatly improved while the consumption of Pt is reduced by taking non-noble metal Ni and Pd alloy with lower price as nuclei.

Description

Preparation method of three-element double-layer PdNi @ Pt nanowire
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a preparation method of a catalyst.
Technical Field
With the continuous development of scientific technology, the demand of human beings on energy is continuously increased, and the rapid consumption of petrochemical fuels causes the extreme shortage of natural resources, so that the concentration of greenhouse gases is greatly increased, and the environment is increasingly seriously damaged and polluted, so that the development of alternative energy and green clean energy becomes the main direction for research and discussion of scientists at the present stage. Among them, proton exchange membrane fuel cells are widely studied in the scientific and engineering fields due to their advantages of high efficiency, high stability, zero greenhouse gas emission, etc. The fuel cell is an electrochemical conversion device, which can convert chemical energy into electric energy, heat and water by reacting with oxidant in the presence of a catalyst, wherein the catalyst influences the speed of reaction and plays a decisive role in the working efficiency of the fuel cell, so scientists take the preparation of efficient and stable catalysts as the important research content of the fuel cell. Among them, platinum is considered to be the most efficient, most valuable and widely studied catalyst, but since platinum element is very small in content in nature and expensive, scientists have focused on reducing the amount of platinum used while improving the performance of platinum.
In the course of several decades of research, scientists have prepared platinum-based nanostructured catalysts with various morphologies, such as core-shell, nano-particles, nano-wires, nano-crystals, etc., and at the same time, they have found that metals, such as palladium, nickel, etc., can improve the catalytic performance of platinum and can reduce the amount of platinum used, wherein, a thin layer of platinum element is wrapped outside the metal nanostructures with various morphologies, and the resulting M @ Pt core-shell structured catalyst has become an important means for reducing the amount of Pt used and improving the utilization rate of Pt.
Researches show that the core-shell structure catalyst prepared at the present stage has more particles or cubes, but in electrochemical catalysis, the superfine single crystal nanowires are made to stand out in the shapes of various catalysts by using the ultrahigh length-diameter ratio, the ultrahigh specific surface area and the high electron transmission speed of the superfine single crystal nanowires, and the core-shell structure nanowires at the present stage take single-element metal nanowires as cores, so that the synergistic effect of a core template is limited, the catalytic activity of metal platinum at an outer layer is influenced, and the catalyst cost with noble metal as the core is higher.
Disclosure of Invention
The invention aims to provide a preparation method of a three-element double-layer PdNi @ Pt nanowire, which can reduce the use amount of Pt and greatly improve the activity of a catalyst. The preparation method mainly comprises the steps of preparing the PdNi alloy nanowire by a hydrothermal method, and then wrapping a layer of Pt outside the nanowire by a reducing agent method to prepare the PdNi @ Pt one-dimensional material.
The three-element double-layer PdNi @ Pt nanowire is a one-dimensional nanowire with a nuclear shell structure, wherein a layer of Pt is wrapped on a PdNi alloy nanowire with the diameter of 4.8 nm.
The preparation method of the three-element double-layer PdNi @ Pt nanowire comprises the following steps:
(1) preparing PdNi alloy nanowires with the diameter of 4.8nm by using a hydrothermal solvent method:
adding 30-40 mg of PdCl into every 10m of L distilled water2Powder and NiCl2Powder proportion of PdCl2Powder and NiCl2Mixing the powder, dissolving in distilled water, performing ultrasonic dispersion uniformly to prepare mixed metal chloride solution, standing for 5-8 min for later use, wherein the PdCl is PdCl2Powder and NiCl2The mass percent of the powder is 2-3.7: 1-1.5, adding 750-970 mg of PVP and NaI into L per 10m of distilled water, dissolving the PVP and the NaI into the distilled water, wherein the mass percent of the PVP and the NaI is 4.25-6.25: 1-2, conducting ultrasonic treatment for 1-2 min to enable the PVP and the NaI to be uniformly dispersed, sucking the supernatant of the mixed metal chloride solution by a liquid transfer gun, adding the mixed metal chloride solution into the mixed solution of the PVP and the NaI, stirring uniformly, pouring the mixed solution into a polytetrafluoroethylene lining of a hydrothermal kettle, covering and screwing the polytetrafluoroethylene lining, placing the kettle into a muffle furnace at 200-240 ℃ for reaction for 2-3 h, conducting centrifugal cleaning for 2-3 times at 8000-9500 r/min by using an ethanol and acetone mixed solution with the volume ratio of 2: 1 after cooling, preparing 4.8nm PdNi alloy nanowires, and dissolving the PdNi alloy nanowires into the distilled water according to the ratio of adding 14-18 mg of L per 10m of distilled water for standby.
(2) Preparing PdNi @ Pt core-shell structure nanowires:
the volume ratio of the PdNi alloy nanowire solution to the ethylene glycol solvent is 1-1.6: 4-6, slowly adding the PdNi alloy nanowire solution obtained in the step (1) into an ethylene glycol solvent, magnetically stirring at the temperature of 50-80 ℃ for 5-10 min at the stirring speed of 200-300 r/min, and then mixing the mixed solution of the PdNi alloy nanowire solution and the ethylene glycol solvent with H2PtCl6The volume ratio of (A) to (B) is 50-76: 1-4, adding H with the concentration of 4.5-8 mM dropwise by using a liquid-transferring gun2PtCl6And stirring for 8-12 h at 50-80 ℃, finally centrifugally cleaning for 2-3 times by using ethanol at 8000-9500 r/min, and drying in a 70 ℃ blast drying oven to obtain the ternary double-layer PdNi @ Pt nanowire.
Compared with the prior art, the invention has the following advantages:
(1) the method is simple, and the three-element double-layer PdNi @ Pt nanowire is prepared.
(2) The cost of the catalyst is reduced, and the activity of the catalyst is greatly improved while the dosage of Pt is reduced by taking non-noble metal Ni and Pd alloy with lower price as nuclei.
Drawings
FIG. 1 is a TEM image of PdNi alloy nanowires synthesized in example 1 of the present invention.
FIG. 2 is a TEM image of PdNi @ Pt core-shell structure nanowire prepared in example 2 of the present invention, wherein a is a TEM image at 200nm, and b is a TEM image at 50 nm.
FIG. 3 is an elemental analysis chart of the PdNi alloy nanowire prepared in embodiment 3 of the present invention.
FIG. 4 is an HRTEM image of PdNi @ Pt nanowire prepared in example 3 of the present invention.
Detailed Description
Example 1
Weighing 10mg of PdCl2And 5mg NiCl2Dissolving the powder in 5m L distilled water, ultrasonically dispersing for uniform, standing for 5min, dissolving 850mg PVP and 200mg NaI in 14m L distilled water, ultrasonically dispersing for 1min, sucking the supernatant of the mixed solution of metal chloride with a pipette, adding into the mixed solution of PVP and NaI, stirring, pouringPutting the mixture into a polytetrafluoroethylene lining of a hydrothermal kettle, covering and screwing the mixture, then placing the mixture into a 200 ℃ muffle furnace for reaction for 2 hours, cooling the mixture, then centrifugally cleaning the mixture for 2 times at 8000r/min by using a mixed solution of ethanol and acetone with the volume ratio of 2: 1 to prepare 8.16mg of PdNi alloy nanowires with the diameter of 4.8nm, and finally dissolving the PdNi alloy nanowires in 5m L distilled water for later use.
Taking 5m L PdNi alloy nanowire solution obtained in the step (1), slowly adding the solution into 20m L ethylene glycol solvent, magnetically stirring the solution at 50 ℃ for 5min at the stirring speed of 200r/min, and dropwise adding H with the concentration of 4.5mM and the concentration of 0.5m L into the solution by using a liquid-transferring gun2PtCl6And stirring for 8h at 50 ℃, finally centrifugally cleaning for 2 times by using ethanol at 8000r/min, and drying in a 70 ℃ blast drying oven to obtain the ternary element double-layer PdNi @ Pt nanowire.
As shown in fig. 1, the prepared core template is PdNi alloy nanowires, the average diameter of which is 4.8 nm.
Example 2
13.7mg of PdCl are weighed out2And 4.1mg NiCl2Dissolving the powder in 5.5m L distilled water, performing ultrasonic dispersion uniformly, standing for 6min, weighing 1000mg PVP, dissolving 300mg NaI in 15m L distilled water, performing ultrasonic dispersion for 1.5min, sucking the supernatant of the metal chloride mixed solution by using a liquid transfer gun, adding the supernatant into the mixed solution of the PVP and NaI, stirring uniformly, pouring into a polytetrafluoroethylene lining of a hydrothermal kettle, covering and screwing the kettle, placing the kettle in a muffle furnace at 210 ℃ for reaction for 2.5h, cooling, performing centrifugal cleaning for 3 times by using an ethanol and acetone mixed solution with a volume ratio of 2: 1 at 9000r/min to prepare 9.09mg PdNi alloy nanowires with the diameter of 4.8nm, and finally dissolving in 6.5m L distilled water for later use.
Taking 6.5m L PdNi alloy nanowire solution obtained in the step (1), slowly adding the solution into 25.5m L ethylene glycol solvent, carrying out magnetic stirring at 60 ℃ for 7min at the stirring speed of 260r/min, and then dropwise adding H with the concentration of 5mM and the concentration of 1.0m L by using a liquid-moving gun2PtCl6And stirring for 10h at 60 ℃, finally centrifugally cleaning for 3 times by using ethanol at 9000r/min, and drying in a 70 ℃ blast drying oven to obtain the ternary element double-layer PdNi @ Pt nanowire.
As shown in FIG. 2, the PdNi @ Pt nanowire with a regular morphology is prepared.
Example 3
16.5mg of PdCl are weighed out2And 5.5mg NiCl2Dissolving the powder in 6m L distilled water, performing ultrasonic dispersion uniformly, standing for 7min, weighing 1150mg PVP, and 350mg NaI in 16m L distilled water, performing ultrasonic dispersion for 1.5min, sucking the supernatant of the metal chloride mixed solution by using a pipette, adding the supernatant into the mixed solution of the PVP and NaI, stirring uniformly, pouring into a polytetrafluoroethylene lining of a hydrothermal kettle, capping, screwing, placing in a 230 ℃ muffle furnace for reaction for 2.8h, cooling, performing centrifugal cleaning for 2 times at 8800r/min by using an ethanol and acetone mixed solution with the volume ratio of 2: 1 to prepare 12.35mg PdNi alloy nanowires with the diameter of 4.8nm, and finally dissolving the PdNi alloy nanowires in 7m L distilled water for later use.
Taking 7m L PdNi alloy nanowire solution obtained in the step (1), slowly adding the solution into 27m L ethylene glycol solvent, magnetically stirring for 8min at 70 ℃, wherein the stirring speed is 280r/min, and then dropwise adding 1.5m L H with the concentration of 6.5mM by using a liquid-transferring gun2PtCl6And stirring for 11h at 70 ℃, finally centrifugally cleaning for 2 times by using ethanol at 8800r/min, and drying in a 70 ℃ blast drying oven to obtain the ternary element double-layer PdNi @ Pt nanowire.
As shown in FIG. 3, the PdNi alloy nanowires prepared have uniform element distribution to form PdNi alloy.
Example 4
18.5mg of PdCl are weighed out2And 7.5mg NiCl2Dissolving the powder in 6.5m L distilled water, performing ultrasonic dispersion uniformly, standing for 8min, dissolving 1250mg PVP and 400mg NaI in 17m L distilled water, performing ultrasonic dispersion for 2min, sucking the supernatant of the metal chloride mixed solution by using a liquid transfer gun, adding the supernatant into the mixed solution of the PVP and NaI, stirring uniformly, pouring into a polytetrafluoroethylene lining of a hydrothermal kettle, covering, screwing, placing in a muffle furnace at 240 ℃ for reaction for 3h, cooling, performing centrifugal cleaning for 3 times by using a mixed solution of ethanol and acetone with a volume ratio of 2: 1 at 9500r/min to prepare 14.44mg PdNi alloy nanowires with the diameter of 4.8nm, and finally dissolving in 8m L distilled water for later use.
Taking 8m L of the PdNi alloy nanowire solution obtained in the step (1),slowly adding into 30m L ethylene glycol solvent, magnetically stirring at 80 deg.C for 10min at stirring speed of 300r/min, and dropwise adding 2m L H with concentration of 8mM by using pipette2PtCl6And stirring for 12h at 80 ℃, finally centrifugally cleaning for 3 times by using ethanol at 9500r/min, and drying in a 70 ℃ blast drying oven to obtain the ternary element double-layer PdNi @ Pt nanowire.
As shown in FIG. 4, the prepared PdNi @ Pt core-shell structure nanowire is well-defined in level, the core is PdNi alloy, and the outer layer is Pt.

Claims (2)

1. A three-element double-layer PdNi @ Pt nanowire is characterized in that: the PdNi alloy nanowire with the diameter of 4.8nm is wrapped by a layer of Pt core-shell structure one-dimensional nanowire, and the preparation method comprises the following steps:
(1) preparing PdNi alloy nanowires with the diameter of 4.8nm by using a hydrothermal solvent method:
adding 30-40 mg of PdCl into every 10m of L distilled water2Powder and NiCl2Powder proportion of PdCl2Powder and NiCl2Mixing the powder, dissolving in distilled water, performing ultrasonic dispersion uniformly to prepare mixed metal chloride solution, standing for 5-8 min for later use, wherein the PdCl is PdCl2Powder and NiCl2Adding 750-970 mg of mixture of PVP and NaI into L mass percent of distilled water per 10m, dissolving the PVP and NaI into the distilled water, wherein the mass percent of the PVP and NaI is 4.25-6.25: 1-2, performing ultrasonic treatment for 1-2 min to uniformly disperse the PVP and NaI, sucking the supernatant of the mixed metal chloride solution by using a liquid transfer gun, adding the mixture into the mixed solution of the PVP and NaI, uniformly stirring, pouring the mixture into a polytetrafluoroethylene lining of a hydrothermal kettle, covering and screwing the polytetrafluoroethylene lining, reacting in a muffle furnace at 200-240 ℃ for 2-3 h, cooling, performing centrifugal cleaning for 2-3 times at 8000-9500 r/min by using an ethanol and acetone mixed solution with the volume ratio of 2: 1 to prepare 4.8nm PdNi alloy nanowires, and dissolving the PdNi alloy nanowires into the distilled water according to the ratio of adding 14-18 mg of PdNi alloy nanowires into L mass percent of distilled water per 10m for later use;
(2) preparing PdNi @ Pt core-shell structure nanowires:
according to PdNi alloy nanowire solution and ethylene glycol solventThe volume ratio is 1-1.6: 4-6, slowly adding the PdNi alloy nanowire solution obtained in the step (1) into an ethylene glycol solvent, magnetically stirring at the temperature of 50-80 ℃ for 5-10 min at the stirring speed of 200-300 r/min, and then mixing the mixed solution of the PdNi alloy nanowire solution and the ethylene glycol solvent with H2PtCl6The volume ratio of (A) to (B) is 50-76: 1-4, adding H with the concentration of 4.5-8 mM dropwise by using a liquid-transferring gun2PtCl6And stirring for 8-12 h at 50-80 ℃, finally centrifugally cleaning for 2-3 times by using ethanol at 8000-9500 r/min, and drying in a 70 ℃ blast drying oven to obtain the ternary double-layer PdNi @ Pt nanowire.
2. The preparation method of the three-element double-layer PdNi @ Pt nanowire disclosed by claim 1 is characterized by comprising the following steps of:
(1) preparing PdNi alloy nanowires with the diameter of 4.8nm by using a hydrothermal solvent method:
adding 30-40 mg of PdCl into every 10m of L distilled water2Powder and NiCl2Powder proportion of PdCl2Powder and NiCl2Mixing the powder, dissolving in distilled water, performing ultrasonic dispersion uniformly to prepare mixed metal chloride solution, standing for 5-8 min for later use, wherein the PdCl is PdCl2Powder and NiCl2Adding 750-970 mg of mixture of PVP and NaI into L mass percent of distilled water per 10m, dissolving the PVP and NaI into the distilled water, wherein the mass percent of the PVP and NaI is 4.25-6.25: 1-2, performing ultrasonic treatment for 1-2 min to uniformly disperse the PVP and NaI, sucking the supernatant of the mixed metal chloride solution by using a liquid transfer gun, adding the mixture into the mixed solution of the PVP and NaI, uniformly stirring, pouring the mixture into a polytetrafluoroethylene lining of a hydrothermal kettle, covering and screwing the polytetrafluoroethylene lining, reacting in a muffle furnace at 200-240 ℃ for 2-3 h, cooling, performing centrifugal cleaning for 2-3 times at 8000-9500 r/min by using an ethanol and acetone mixed solution with the volume ratio of 2: 1 to prepare 4.8nm PdNi alloy nanowires, and dissolving the PdNi alloy nanowires into the distilled water according to the ratio of adding 14-18 mg of PdNi alloy nanowires into L mass percent of distilled water per 10m for later use;
(2) preparing PdNi @ Pt core-shell structure nanowires:
PdNi alloy nanowire solution and BThe volume ratio of the glycol solvent is 1-1.6: 4-6, slowly adding the PdNi alloy nanowire solution obtained in the step (1) into an ethylene glycol solvent, magnetically stirring at the temperature of 50-80 ℃ for 5-10 min at the stirring speed of 200-300 r/min, and then mixing the mixed solution of the PdNi alloy nanowire solution and the ethylene glycol solvent with H2PtCl6The volume ratio of (A) to (B) is 50-76: 1-4, adding H with the concentration of 4.5-8 mM dropwise by using a liquid-transferring gun2PtCl6And stirring for 8-12 h at 50-80 ℃, finally centrifugally cleaning for 2-3 times by using ethanol at 8000-9500 r/min, and drying in a 70 ℃ blast drying oven to obtain the ternary double-layer PdNi @ Pt nanowire.
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CN103178274A (en) * 2013-03-19 2013-06-26 南通大学 Anode catalyst of PdMo/TiO2 nanowire direct methanol fuel cell and preparation method
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CN106925771A (en) * 2017-03-14 2017-07-07 中国科学技术大学先进技术研究院 Ultra-fine PtRh nano wires and its method for preparing catalyst, application

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